26 results about "Antimony trichloride" patented technology

The invention relates to the technical field of metal powder material preparation, and particularly discloses antimony-doped cesium terbium chloride microcrystalline powder and a preparation method thereof. The chemical composition of the microcrystalline powder is Cs < 5 > Tb < 1-x > Sb < x > Cl < 8 >. 6H < 2 > O, wherein x is equal to 0.05 to 0.30. The preparation method comprises the following steps: mixing cesium chloride, terbium chloride hexahydrate and antimony trichloride according to a molar ratio of 5: 0.8: x; adding pyridine hydrochloride as a chlorine element supplement, wherein the dosage of the pyridine hydrochloride is that 0.05-0.20 mmol of Py.HCl is used for every 1 mmol of CsCl; adding stearic acid as a process dispersant; and through combined treatment of mechanical ball milling and freeze drying, antimony-doped cesium-terbium-chlorine microcrystal powder with regular morphology and good dispersibility is obtained. The method is simple in process and mild in condition, particle aggregation can be effectively inhibited, the crystallinity and dispersion uniformity of the powder are improved, and the prepared microcrystal powder shows excellent optical performance.

The application relates to a preparation method of a TiO2 / Sb2O3 / PSAC heterojunction sterilization composite material, which comprises the following steps: 1) adding a cationic surfactant, tetrabutyl titanate, antimony trichloride or antimony pentachloride into deionized water in sequence and stirring until the solution is white; 2) placing a FOSS crucible with coal-tar pitch-based spherical activated carbon into a high-pressure reaction kettle with concentrated nitric acid, heating, washing with deionized water until neutral, and naturally air-drying; 3) placing the dried coal-tar pitch-based spherical activated carbon into the white solution, stirring, finally adding sodium hydroxide, stirring, and then placing into a high-pressure reaction kettle, heating and keeping for a period of time; and naturally cooling, centrifugalizing, washing and drying. The application effectively combines the adsorption performance and the photocatalytic performance of the activated carbon through a hydrothermal one-step in-situ method, increases the mechanical performance, and can have high sterilization efficiency under the excitation of sunlight.

The invention relates to the technical field of electrochemical water treatment, in particular to a preparation method of a self-supporting antimony-doped tin dioxide nanoflower electrode, which comprises the following steps: dissolving trisodium citrate dehydrate and antimony trichloride in absolute ethyl alcohol; then adding water and stannous chloride dehydrate to form a precursor solution; heating the precursor solution, and naturally cooling; after cooling, carrying out solid-liquid separation on the bottom mud, and then cleaning and drying to obtain antimony-doped tin dioxide powder; taking antimony-doped tin dioxide powder, a pore-forming agent and a binder, grinding the materials until the materials are uniformly mixed, and transferring the materials into a tabletting mold for pressure casting to obtain a blank; and calcining the green body to obtain the product. Nano-flower-shaped antimony-doped tin dioxide powder is prepared, in the die casting and sintering process, due to the fact that nano-flower petals of the nano-flower-shaped antimony-doped tin dioxide powder are mutually staggered, a connection mode similar to a mortise and tenon joint mode is formed, and compared with nanospheres, the binding force between the powder is enhanced; and the mechanical strength, the electrochemical active area and the catalytic activity of the electrode are improved.

A simple and efficient method for preparing high-purity rubidium chloride includes the following steps: Adding crude rubidium salt to glacial acetic acid, heating and stirring to dissolve, filtering to remove insoluble impurities, yielding a crude rubidium salt solution in glacial acetic acid; adding a certain amount of antimony trichloride solution to the crude rubidium salt solution in glacial acetic acid, stirring the reaction to obtain a small amount of pale yellow precipitate and solution until the reaction reaches equilibrium, yielding a clear liquid and precipitate, the precipitate being used to prepare high-purity cesium salt; secondary precipitation: adding a certain amount of tin tetrachloride solution in glacial acetic acid to the clear liquid, stirring the reaction to obtain a white precipitate and solution; standing, filtering, and washing: cooling and standing the solution until the reaction reaches equilibrium, filtering, washing the precipitate with glacial acetic acid, yielding a precipitate and washing liquid; double salt decomposition: adding high-purity water to the precipitate to form a slurry, then adding ammonia to adjust the pH value, filtering to obtain tin hydroxide precipitate and rubidium chloride solution; sending the filtrate for testing: evaporating the qualified rubidium chloride solution to dryness, calcining to obtain rubidium chloride; recrystallization: obtaining the high-purity rubidium chloride product. It has the advantages of effectively removing cesium ions from crude rubidium salt and avoiding the influence of alkali metal ions on the purity of the final product, without loss, and with high product purity.

This application relates to the field of zinc-based battery technology and discloses a method for preparing a negative electrode current collector for zinc-nickel batteries. The negative electrode current collector includes a three-dimensional porous copper substrate and a tin-antimony functional layer formed on the surface of the substrate. The preparation method involves immersing the three-dimensional porous copper substrate in a functional deep eutectic solvent and performing a low-temperature in-situ chemical conversion reaction at a preset temperature of 80–120°C. The functional deep eutectic solvent is prepared from choline chloride, urea, anhydrous stannous chloride as a tin source, anhydrous antimony trichloride as an antimony source, and imidazole as a reaction regulator. This invention utilizes the copper substrate as a reducing agent to generate a tin-antimony functional layer that is firmly bonded to the substrate in situ. This method is a one-pot operation with a simple process and no wastewater generation. The obtained current collector can effectively inhibit zinc dendrite growth, improving the cycle life and safety of the battery.

The invention discloses a preparation method of an antimony trioxide composite flame retardant, which is specifically implemented according to the following steps: pretreating a catalytic cracking poising agent to obtain a poising agent solution, and adding antimony trichloride into hydrochloric acid; dropwise adding an antimony trichloride solution into the poising agent solution, and stirring for 3-5 hours to obtain a first mixed solution; standing to enable precipitates in the first mixed solution to settle to the bottom, clarifying supernatant liquid, then pouring out the supernatant liquid, and filtering bottom turbid liquid to obtain a first filter cake; adding water into the first filter cake, dispersing to obtain a first turbid solution, adding an alkaline solution into the first turbid solution, neutralizing to obtain a second turbid solution, filtering the second turbid solution to obtain a second filter cake, washing the second filter cake, and drying to obtain the antimony trioxide composite flame retardant. The preparation method of the antimony trioxide composite flame retardant is simple in process, low in raw material cost, high in additional value and environmentally friendly.

The invention relates to the technical field of antimony extraction, in particular to an antimony ore smelting process which comprises the following preparation steps: S1, mixing crushed ultralow antimony ore with a sulfur source and a reducing agent in an inert atmosphere, and performing microwave-assisted sulfuration roasting at 450-550 DEG C to convert antimony tetroxide into volatile antimony trisulfide; s2, mixing the vulcanized calcine with calcium chloride, bentonite and water to prepare pellets of 10-15 mm, performing chloridizing roasting in a weak oxidizing atmosphere at 650-750 DEG C, and condensing volatile gas to obtain antimony trichloride; and S3, antimony trichloride is fed into a molten pool smelting furnace, a reducing agent and oxygen-enriched air are sprayed, metal antimony and chlorine-containing flue gas are obtained through reduction smelting at the temperature of 1150-1250 DEG C, and the flue gas is recycled to prepare calcium chloride for recycling. According to the method, through a low-temperature vulcanization-chlorination-molten pool reduction closed-loop metallurgical system, efficient enrichment and short-process extraction of antimony are achieved, and the metal recovery rate is gt; the cyclic utilization rate of calcium chloride is gt; the method has the advantages of being high in recovery rate, low in energy consumption, clean and environmentally friendly, and is suitable for recycling treatment of the ultralow-grade antimony ore.

The present invention relates to an improved process for the preparation of 2-bromo-5-fluorobenzotrifluoride comprising, reacting 3-fluorobenzotrifluoride with brominating agent in the presence of antimony catalyst selected from antimony trichloride (SbCl3), antimony pentachloride (SbCl5) or mixture(s) thereof, to provide 2-bromo-5- fluorobenzotrifluoride with higher yield and purity

The invention relates to the field of heat-insulating glass preparation, in particular to a heat-insulating glass preparation method based on E-51 / ATO, which comprises the following steps: 1, pouring tin tetrachloride pentahydrate and antimony trichloride as precursors into a stainless steel high-pressure kettle with a para-polyphenol lining, and sealing to obtain an ATO dispersion solution; 2, the ATO dispersion solution is centrifuged and washed with ethyl alcohol and deionized water respectively, and dried nanometer ATO powder is obtained; 3, weighing E-51, an amine curing agent and acetone, uniformly mixing, pouring the nano ATO powder, and continuously stirring to obtain uniform ATO / E-51 slurry; and 4, fixing the pretreated glass substrate on a platform, injecting the ATO / E-51 slurry into a spray pen material cup, spraying the ATO / E-51 slurry on the surface of the glass substrate, and drying and curing a sprayed sample to obtain the ATO / E-51 heat-insulating glass with a compact surface structure. ATO nano-particles with the particle size of 10 nm are directly prepared through an optimized solvothermal method, and then agglomeration of the nano-particles is effectively prevented through an accurate mass ratio and high-speed stirring synergistic dispersion process.

The invention discloses a preparation method of an antimony oxychloride composite flame retardant, which is characterized by specifically comprising the following steps: pretreating a catalytic cracking equilibrium agent to obtain an equilibrium agent solution, and adding antimony trichloride into hydrochloric acid to obtain an antimony trichloride solution; dropwise adding an antimony trichloride solution into the poising agent solution, and stirring for 3-5 hours to obtain a first mixed solution; adding an alkaline solution into the first mixed solution to neutralize until the pH is 7-8, standing and filtering to obtain a filter cake; and washing the filter cake, and drying to obtain the antimony oxychloride-based composite flame retardant. The preparation method of the antimony oxychloride composite flame retardant is simple in process, low in raw material cost, high in additional value and environment-friendly, and solves the problem of recovery of a catalytic cracking equilibrium agent.

The invention discloses a preparation method of a high-crystallinity Sb2S3 antimony sulfide film, which not only can be applied to a PEC photocathode, but also can be applied to the fields of solar cells, photoelectric detection and the like. According to the method, 2, 4, 6-trichlorophenol is used as an additive and dissolved in acetone together with antimony trichloride, and the high-quality Sb2S3 antimony sulfide thin film is obtained through chemical bath deposition. According to the method, the Sb2S3 precursor and the acetone solvent serve as raw materials, the interaction between Cl atoms and Sb atoms at the tail ends of 2, 4, 6-trichlorophenol molecules is utilized, the intermolecular interaction between the Sb2S3 precursor and the acetone solvent can be enhanced through the interaction, the number of Sb2S3 crystal nucleuses is reduced along with reduction of the supersaturation degree, and growth of the crystal nucleuses is further promoted. And the crystallization peak intensity is enhanced from 150 to 500. Meanwhile, the Fermi level of semiconductor antimony sulfide is reduced, P-type conductivity is enhanced, and therefore the performance of the antimony sulfide photoelectric cathode is improved.

The present invention relates to the field of inorganic materials, and in particular to a method for preparing clustered antimony trioxide. The method comprises the following steps: adding antimony trichloride to an organic solvent consisting of ethanol and n-butanol, adding a surfactant and mixing, dropping deionized water, and adjusting the pH of the system to 1-2 to obtain a mixed solution. The mixed solution is transferred to a polytetrafluoroethylene-lined autoclave, sealed, heated to 120-150°C, and reacted for 5-10 hours. After returning to room temperature, the pH of the reaction solution is adjusted to 8-9 with an alkaline solution, stirred for 10-60 minutes, and then the precipitate is collected, washed, and dried. The clustered antimony trioxide prepared by the present invention is used as an active material and can significantly improve the electrochemical performance of a lithium-ion battery.

The present application relates to triethyl antimony processing technical field, especially in kind of preparation triethyl antimony, including the following steps: under the protection of inert gas to the reaction bottle raw material antimony trichloride and ether solvent is added, and the atmospheric pressure reflux device is installed, and the stirring is started;Ethyl lithium ether solution is added dropwise to the reaction bottle, after dropwise addition is completed, 70~80 ℃ stirring reaction is kept for 3~6h;After the stirring reflux is finished, the solvent ether is distilled out first, and the triethyl antimony initial product is obtained;The vacuum distillation device is installed, and the triethyl antimony crude product is obtained by vacuum distillation;The obtained triethyl antimony crude product is subjected to twice vacuum rectification, and high-purity triethyl antimony is obtained, and the purity reaches 6N by nuclear magnetic resonance, ICP detection.Pure triethyl antimony is generated by the reaction of ethyl lithium and antimony trichloride under the protection of inert gas, the preparation method is safe and efficient, simple operation, raw material is easy to obtain, no by-product, high yield and high purity product.

The invention relates to the field of inorganic materials, in particular to a preparation method of antimony trioxide nanoparticles, which specifically comprises the following steps: uniformly mixing antimony sulfide ore with inorganic fused salt, transition metal oxide and a carbon material, grinding into powder, pressing the powder into blocks, smelting to obtain molten liquid, separating crude antimony from the molten liquid, dissolving the crude antimony with hydrochloric acid, and drying to obtain the antimony trioxide nanoparticles. Adding high-purity antimony powder, stirring and reacting to obtain an antimony trichloride crude solution, filtering the antimony trichloride crude solution, adding ammonia water and ionic liquid into the obtained filtrate, stirring and reacting, collecting a product, and drying. The inorganic molten salt contains metal fluoride, and antimony trioxide prepared by the method not only has a cubic crystal form, but also has a nano size, and is higher in economic added value and wider in application prospect.

The invention relates to a Sn-Se-Sb thin film negative electrode material and a preparation method thereof.The preparation method comprises the steps that a certain amount of sodium citrate, seleninic acid, ethylene glycol and stannic chloride are sequentially added into deionized water and stirred to be completely dissolved, and a solution A is obtained; adding antimony trichloride into absolute ethyl alcohol, and stirring until the antimony trichloride is completely dissolved to obtain a solution B; mixing the prepared solution A and the prepared solution B to obtain an electroplating solution C; and placing the electrolyte C in an electrolytic cell, taking a copper foil as a working electrode, a platinum sheet as a counter electrode and a mercury / mercurous sulfate electrode as a reference electrode, connecting an electrochemical workstation, setting and applying alternating voltage at room temperature, depositing for a certain time, and circularly depositing for 7 times according to the alternating voltage, thereby obtaining the Sn-Se-Sb film negative electrode material on the surface of the copper foil. The Sn-Se-Sb film negative electrode material disclosed by the invention has the advantages of high specific capacity, good cycling stability and rate capability, and the preparation method is simple, low in cost, environment-friendly and easy for large-scale production.

The present invention belongs to the field of preparation and application of metal materials and relates to a class of Cl / Br halogen-doped ionic antimony complexes and their preparation methods and applications. The general structural formula of the complex is shown below: #imgabs0#, wherein R is methyl, ethyl, n-propyl or n-butyl; and x=0, 1, 2, 3, 4 or 5. The preparation method comprises the following steps: adding a benzylamine salt and antimony trichloride or antimony tribromide to a solvent in a molar ratio, reacting the mixture, and using ether as a reverse solvent to obtain a single crystal of the target product; or adding a benzylamine salt and antimony trichloride or antimony tribromide to a solvent in a molar ratio, and heating the mixture to obtain a single crystal of the target product. The luminescence properties of the material can be controlled by varying the halogen type or organic cation in the complex. Due to the advantages of the antimony complex, such as high stability, simple preparation, and high-efficiency, short-life luminescence, the ionic antimony complex has a wide range of uses and can be applied to fields such as X-ray imaging and lighting displays.

The application discloses a photovoltaic self-cleaning coating with heat insulation and antistatic functions and a preparation method thereof, and relates to the technical scheme that: nano zinc oxide particles, water and ethanol are mixed to prepare a nano zinc oxide dispersion liquid; a magnesium chloride and ammonium fluoride aqueous solution is added into the nano zinc oxide dispersion liquid, the zinc oxide core is removed after reaction, and a magnesium fluoride emulsion is obtained after purification; antimony trichloride and tin tetrachloride pentahydrate are sequentially added into the acidified magnesium fluoride emulsion, a hollow MgF2@ATO sol is obtained after reaction and purification; tetraethyl orthosilicate is dissolved in the hollow MgF2@ATO sol, and nitric acid aqueous solution is added, stirring is conducted, and aging is carried out to prepare a MgF2@ATO composite sol; an acid hydrolysis mother liquor, the MgF2@ATO composite sol, ethanol, a nitric acid solution and deionized water are mixed, and are coated on a substrate, and a photovoltaic self-cleaning coating is obtained after solidification; the coating can be solidified at room temperature, has low preparation cost, is suitable for industrialized production and application, and the paint film has high light transmittance, hardness, adhesion and antistatic property, and excellent water resistance, weather resistance and heat insulation performance.

The application belongs to the field of antimony rectification devices, and particularly relates to an antimony purification rectification device, which comprises a rectification tower, a plurality of first tower plates and second tower plates are fixedly arranged in the rectification tower, the first tower plate comprises a fixed plate fixedly arranged in a steam pipeline and a lifting plate movably arranged below the fixed plate, a height adjusting assembly is arranged on the side of the lifting plate, the height adjusting assembly comprises a Z-shaped shaft, one end of the Z-shaped shaft is slidably arranged in a sliding groove, the lifting plate is lowered, and a certain distance is kept between the fixed plate and the lifting plate, the space generated by the distance is a sealing space, the gas formed by antimony trichloride in the rectification tower is transmitted upwards through a steam passage assembly, the transmission of the gas does not pass through the space between the fixed plate and the lifting plate, the transmission space of the steam is reduced, and the transmission efficiency is improved.

The application provides an anode membrane assembly for treating high-salt organic wastewater and a preparation method thereof, and belongs to the technical field of water treatment. The preparation method of the anode membrane assembly comprises the following steps: (1) cleaning and etching of a titanium mesh substrate; (2) citric acid and ethylene glycol are poured into a beaker, tin tetrachloride SnCl4.5H2O and antimony trichloride SbCl3 are added while water bath heating, stirring and maintaining water bath heating to form a sol-gel; (3) the substrate is immersed in the sol-gel, and then drying is carried out in an electric heating air drying oven, the above steps are repeated, and the immersed and coated titanium mesh is placed into a muffle furnace for high-temperature calcination to obtain a titanium substrate tin-antimony anode membrane; (4) two pieces of the titanium substrate tin-antimony anode membrane are fixed on the two sides of a PVC membrane support respectively, and ABS glue is used for bonding and sealing at the edge, so that the anode membrane assembly is obtained. The application solves the technical problem that the high Cl ‑ concentration in high-salt wastewater affects the removal of organic matters by electro-oxidation.

The invention discloses a method for removing arsenic and recovering precious metals from high-arsenic and high-antimony soot, which comprises the following steps: firstly, carrying out acid leaching on the high-arsenic and high-antimony soot, and controlling the acid leaching condition to obtain leaching residues and a leaching solution; performing heavy removal on the leachate to obtain heavy-removed liquid and a small amount of heavy-removed slag, and performing arsenic removal on the heavy-removed liquid to obtain arsenic slag and arsenic-removed liquid; and carrying out reduction cooling on the arsenic-removed liquid to obtain cooled slag and a crystallized liquid, carrying out continuous reduced pressure distillation on the crystallized liquid, and controlling distillation conditions to obtain the high-purity antimony trichloride. The method provided by the invention can greatly improve the arsenic-antimony separation efficiency, especially can reduce the loss of antimony when treating high-arsenic and high-antimony soot, and has the advantages of simple process and strong applicability. The method can avoid adverse effects on the environment, efficiently and comprehensively recover gold and silver in the high-arsenic and high-antimony smoke dust, realize high-valued utilization of antimony, and greatly improve the utilization rate of the high-arsenic and high-antimony smoke dust.

The invention relates to the technical field of zinc-based batteries, and discloses a zinc-nickel battery negative electrode current collector preparation method, and the negative electrode current collector comprises a three-dimensional porous copper base material and a tin-antimony functional layer formed on the surface of the base material. The preparation method comprises the following steps: immersing the three-dimensional porous copper base material in a functional deep eutectic solvent, and carrying out low-temperature in-situ chemical conversion reaction at a preset temperature of 80-120 DEG C; the functional deep eutectic solvent is prepared from choline chloride, urea, anhydrous stannous chloride serving as a tin source, anhydrous antimony trichloride serving as an antimony source and imidazole serving as a reaction regulating agent. The copper base material is used as a reducing agent, and the tin-antimony functional layer firmly combined with the base material is generated in situ. The method is operated by a one-pot method, the process is simple, and no wastewater is generated; the prepared current collector can effectively inhibit the growth of zinc dendrites, and the cycle life and safety of the battery are improved.

The invention discloses scandium-antimony electroplating liquid, a negative electrode three-dimensional current collector and application of the scandium-antimony electroplating liquid, and belongs to the technical field of battery materials. The scandium-antimony electroplating solution comprises the following components: 20 to 100g / L of antimony trichloride, 1 to 10g / L of scandium trichloride, 150 to 220g / L of citric acid, 100 to 180g / L of potassium citrate and 20 to 100g / L of ethanol. The problem that the battery performance is not ideal due to the concentration polarization phenomenon in the current collector with the three-dimensional skeleton structure can be solved.

This invention provides a method for preparing and applying an inorganic-organic mixed ammonium modified sandwich-type dinuclear uranium-tungsten-antimonate visible light photocatalyst. Belonging to the field of catalyst technology, the method for preparing an inorganic-organic mixed ammonium modified sandwich-type dinuclear uranium-tungsten-antimonate visible light photocatalyst includes the following steps: sodium tungstate dihydrate, ammonium chloride, tetramethylammonium bromide, antimony trichloride, and uranyl nitrate hexahydrate are sequentially added to a 100 mL beaker; 30-100 mL of deionized water is added to the beaker, and then... (The sentence is incomplete and requires further context to translate accurately.) ‑1 Adjust the pH of the solution with HCl solution to pH 2-5; after stirring the reaction solution in step S2 evenly, place it in a water bath and heat it at 60-100℃ for 3 hours; after taking out the reaction solution in step S3 and cooling it to room temperature, filter it and evaporate the filtrate in the open at room temperature.

This invention relates to the field of inorganic materials, specifically to a preparation process for electronic-grade antimony trioxide. The process involves dissolving antimony trichloride in anhydrous ethanol to obtain solution A; dissolving a thermosensitive polymer in deionized water and adjusting the pH to 9-10 with ammonia to obtain solution B; heating solution B to above 50°C; adding solution A to solution B; stirring the reaction; restoring to room temperature; collecting the product; washing; and drying. The antimony trioxide prepared by this invention exhibits excellent electrochemical performance and demonstrates superior cycle performance in lithium batteries.

The invention provides a preparation method of a Cu2Sb / NC electrocatalyst and a zinc-air battery. The preparation method comprises the following steps: preparing a Cu-ZIF-8 precursor; preparing an N, N-dimethylformamide solution of antimony trichloride and phenanthroline, adding the Cu-ZIF-8 precursor, stirring, centrifuging, and drying to obtain Cu-ZIF-8 (at) SbCl3 powder; and putting the powder into a tubular furnace for high-temperature pyrolysis to obtain the Cu2Sb / NC electrocatalyst. And the powder is put into a tubular furnace to be subjected to high-temperature pyrolysis, and Cu2Sb / NC is obtained. The catalyst has excellent oxygen reduction reaction (ORR) activity, shows high power density as an air cathode of a zinc-air battery, and has a wide application prospect in the field of zinc-air batteries.

The application relates to the technical field of metal powder material preparation, and particularly discloses a kind of antimony-doped cesium terbium chloride microcrystalline powder and a preparation method thereof.The chemical composition of the microcrystalline powder is Cs5Tb 1‑ x Sb x Cl8.6H2O, wherein x=0.05-0.30.The preparation method comprises the following steps: mixing cesium chloride, terbium chloride hexahydrate and antimony trichloride according to a molar ratio of 5:0.8:x; adding pyridine hydrochloride as a chlorine element supplement, wherein the amount of pyridine hydrochloride is 0.05-0.20 mmol per 1 mmol of CsCl; adding stearic acid as a process dispersant; and performing mechanical ball milling and freeze-drying combined treatment to obtain antimony-doped cesium terbium chloride microcrystalline powder with regular morphology and good dispersity.The application has simple process and mild conditions, can effectively inhibit particle agglomeration, improve the crystallinity and dispersion uniformity of the powder, and the prepared microcrystalline powder exhibits excellent optical performance.